# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Hugo Torrens' 'Maribel Arroyo' 'Sylvain Bernes' 'Luis Villanueva' _publ_contact_author_name 'Dr Hugo Torrens' _publ_contact_author_address ; F. Chemistry Natl. U. Mexico Cd. Universitaria Mexico D.F. 04510 MEXICO ; _publ_contact_author_phone (52)56223724 _publ_contact_author_fax (52)56223724 _publ_contact_author_email Torrens@servidor.unam.mx _publ_requested_coeditor_name ? _publ_contact_letter ? _publ_requested_journal 'Chemical Communications' _publ_section_title ; Evolution of [Pt(SRf)2(PPh2-n(C6F5)n+1)2] (n=0 or 1, Rf = C6HF4-4) Through Carbon-Fluorine Bond Activation to [Pt(SRf)2(1,2-C6F4(SRf)(PPh2))] and Chiral [Pt(SRf)2(1,2-C6F4(SRf)(PPh(C6F5)))]. ; data_lv103-2 _database_code_depnum_ccdc_archive 'CCDC 239571' _audit_creation_method SHELXL-97 _audit_creation_date 2003-03-26 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H14 F36 P2 Pt2 S4' _chemical_formula_sum 'C60 H14 F36 P2 Pt2 S4' _chemical_formula_weight 1999.07 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 25.675(2) _cell_length_b 25.675(2) _cell_length_c 19.115(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10912.5(18) _cell_formula_units_Z 6 _cell_measurement_temperature 296(1) _cell_measurement_reflns_used 84 _cell_measurement_theta_min 4.68 _cell_measurement_theta_max 12.29 _exptl_crystal_description hexagonal_plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5688 _exptl_absorpt_coefficient_mu 4.129 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.197 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_process_details '18 psi scans with XSCAnS 2.21 (Fait, 1996)' _exptl_special_details ? _diffrn_ambient_temperature 296(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_source_power 1.5 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_detector 'Scintillation counter' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -6 1 -6 5 0 -6 3 -1 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 13877 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6577 _reflns_number_gt 3631 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'XSCAnS 2.21 (Fait, 1996)' _computing_cell_refinement 'XSCAnS 2.21 (Fait, 1996)' _computing_data_reduction 'XSCAnS 2.21 (Fait, 1996)' _computing_structure_solution 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 28 restraints for the refinement: rings C13 > C18, C25 > C30 and C31 > C36 are restrained to a flat geometry, with C-C bond lengths restrained to 1.39(1) \%A. Bond length C35-F35 is restrained to 1.35(2) \%A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+1.6475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6577 _refine_ls_number_parameters 502 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1528 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.901861(15) 0.656198(16) 0.34365(2) 0.05543(16) Uani 1 1 d . . . P1 P 0.96855(13) 0.68596(14) 0.43326(16) 0.0695(8) Uani 1 1 d . . . S1 S 0.82862(13) 0.63397(14) 0.42844(16) 0.0772(8) Uani 1 1 d . . . S2 S 0.96961(15) 0.67823(16) 0.2500 0.0618(9) Uani 1 2 d S . . S3 S 0.83202(16) 0.62169(17) 0.2500 0.0663(10) Uani 1 2 d S . . C1 C 0.9745(4) 0.7454(5) 0.4884(6) 0.067(3) Uani 1 1 d . . . C2 C 0.9330(5) 0.7649(5) 0.4864(7) 0.094(4) Uani 1 1 d . . . H2A H 0.9007 0.7470 0.4556 0.113 Uiso 1 1 calc R . . C3 C 0.9390(6) 0.8104(6) 0.5295(8) 0.113(5) Uani 1 1 d . . . H3A H 0.9120 0.8244 0.5252 0.136 Uiso 1 1 calc R . . C4 C 0.9828(6) 0.8352(6) 0.5776(7) 0.101(4) Uani 1 1 d . . . H4A H 0.9840 0.8635 0.6090 0.122 Uiso 1 1 calc R . . C5 C 1.0243(6) 0.8188(5) 0.5799(6) 0.091(4) Uani 1 1 d . . . H5A H 1.0560 0.8373 0.6113 0.109 Uiso 1 1 calc R . . C6 C 1.0205(5) 0.7739(5) 0.5351(6) 0.074(3) Uani 1 1 d . . . H6A H 1.0501 0.7632 0.5373 0.089 Uiso 1 1 calc R . . C7 C 0.9514(5) 0.6227(5) 0.4921(7) 0.079(3) Uani 1 1 d . . . C8 C 0.9476(10) 0.5715(7) 0.4643(10) 0.153(7) Uani 1 1 d . . . C9 C 0.9319(12) 0.5215(8) 0.5036(11) 0.188(10) Uani 1 1 d . . . C10 C 0.9190(11) 0.5184(9) 0.5736(10) 0.169(9) Uani 1 1 d . . . C11 C 0.9226(7) 0.5678(7) 0.6017(9) 0.107(5) Uani 1 1 d . . . C12 C 0.9387(5) 0.6183(6) 0.5609(7) 0.078(3) Uani 1 1 d . . . C13 C 1.0465(6) 0.7148(8) 0.4084(7) 0.105(5) Uani 1 1 d D . . C14 C 1.0736(7) 0.7699(8) 0.3749(8) 0.142(8) Uani 1 1 d D . . C15 C 1.1341(8) 0.8079(12) 0.3554(11) 0.217(18) Uani 1 1 d D . . C16 C 1.1669(10) 0.7811(8) 0.3732(11) 0.170(12) Uani 1 1 d D . . C17 C 1.1461(7) 0.7261(9) 0.4044(9) 0.170(11) Uani 1 1 d D . . C18 C 1.0873(7) 0.6961(8) 0.4272(8) 0.106(5) Uani 1 1 d D . . C19 C 0.7652(5) 0.5656(6) 0.4018(6) 0.086(3) Uani 1 1 d . . . C20 C 0.7096(6) 0.5637(6) 0.3960(7) 0.086(4) Uani 1 1 d . . . C21 C 0.6592(7) 0.5114(9) 0.3792(9) 0.128(6) Uani 1 1 d . . . C22 C 0.6577(9) 0.4616(8) 0.3611(12) 0.168(9) Uani 1 1 d . . . H22A H 0.6232 0.4282 0.3443 0.202 Uiso 1 1 calc R . . C23 C 0.7114(10) 0.4632(7) 0.3690(12) 0.154(8) Uani 1 1 d . . . C24 C 0.7645(8) 0.5131(6) 0.3847(10) 0.120(5) Uani 1 1 d . . . C25 C 0.9846(6) 0.6157(7) 0.2500 0.078(5) Uani 1 2 d SD . . C26 C 1.0452(7) 0.6319(9) 0.2500 0.099(6) Uani 1 2 d SD . . C27 C 1.0576(11) 0.5848(10) 0.2500 0.127(9) Uani 1 2 d SD . . C28 C 1.0124(11) 0.5248(10) 0.2500 0.154(13) Uani 1 2 d SD . . H28A H 1.0219 0.4943 0.2500 0.185 Uiso 1 2 calc SR . . C29 C 0.9529(11) 0.5111(9) 0.2500 0.111(7) Uani 1 2 d SD . . C30 C 0.9377(9) 0.5559(7) 0.2500 0.098(6) Uani 1 2 d SD . . C31 C 0.7997(8) 0.6685(12) 0.2500 0.107(7) Uani 1 2 d SD . . C32 C 0.7368(9) 0.6369(12) 0.2500 0.117(9) Uani 1 2 d SD . . C33 C 0.7065(13) 0.6688(13) 0.2500 0.22(2) Uani 1 2 d SD . . C34 C 0.7370(15) 0.7307(13) 0.2500 0.26(4) Uani 1 2 d SD . . H34A H 0.7178 0.7533 0.2500 0.313 Uiso 1 2 calc SR . . C35 C 0.7988(15) 0.7563(13) 0.2500 0.32(4) Uani 1 2 d SD . . C36 C 0.8354(14) 0.7306(12) 0.2500 0.18(2) Uani 1 2 d SD . . F8 F 0.9574(6) 0.5698(5) 0.3952(5) 0.192(6) Uani 1 1 d . . . F9 F 0.9303(10) 0.4736(6) 0.4705(6) 0.332(12) Uani 1 1 d . . . F10 F 0.9077(8) 0.4704(5) 0.6074(6) 0.240(7) Uani 1 1 d . . . F11 F 0.9110(5) 0.5666(4) 0.6690(5) 0.139(3) Uani 1 1 d . . . F12 F 0.9379(3) 0.6635(3) 0.5958(4) 0.108(2) Uani 1 1 d . . . F14 F 1.0402(4) 0.7951(3) 0.3570(5) 0.123(3) Uani 1 1 d . . . F15 F 1.1548(7) 0.8564(7) 0.3216(10) 0.298(13) Uani 1 1 d . . . F16 F 1.2258(4) 0.8048(8) 0.3610(8) 0.266(9) Uani 1 1 d . . . F17 F 1.1783(5) 0.6982(8) 0.4242(7) 0.259(8) Uani 1 1 d . . . F18 F 1.0653(5) 0.6413(7) 0.4564(6) 0.176(5) Uani 1 1 d . . . F20 F 0.7054(3) 0.6131(4) 0.4085(4) 0.109(2) Uani 1 1 d . . . F21 F 0.6059(4) 0.5135(4) 0.3725(6) 0.171(4) Uani 1 1 d . . . F23 F 0.7172(6) 0.4144(4) 0.3537(9) 0.266(8) Uani 1 1 d . . . F24 F 0.8165(4) 0.5119(4) 0.3909(6) 0.159(4) Uani 1 1 d . . . F26 F 1.0901(4) 0.6905(6) 0.2500 0.102(3) Uani 1 2 d S . . F27 F 1.1180(7) 0.6028(8) 0.2500 0.184(7) Uani 1 2 d S . . F29 F 0.9126(8) 0.4549(6) 0.2500 0.180(7) Uani 1 2 d S . . F30 F 0.8820(5) 0.5399(4) 0.2500 0.101(3) Uani 1 2 d S . . F32 F 0.7023(6) 0.5786(11) 0.2500 0.217(10) Uani 1 2 d S . . F33 F 0.6425(10) 0.6349(15) 0.2500 0.331(16) Uani 1 2 d S . . F35 F 0.8247(15) 0.8157(11) 0.2500 0.291(16) Uani 1 2 d SD . . F36 F 0.8921(9) 0.7581(7) 0.2500 0.172(8) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0580(2) 0.0613(3) 0.0496(2) -0.0036(2) -0.0035(2) 0.03179(19) P1 0.0697(18) 0.088(2) 0.0618(19) -0.0186(16) -0.0142(15) 0.0477(16) S1 0.0765(18) 0.099(2) 0.0555(17) -0.0032(16) 0.0096(15) 0.0431(17) S2 0.058(2) 0.065(2) 0.064(2) 0.000 0.000 0.0314(18) S3 0.055(2) 0.088(3) 0.048(2) 0.000 0.000 0.0299(19) C1 0.053(6) 0.086(7) 0.056(7) -0.014(6) -0.015(5) 0.030(6) C2 0.099(9) 0.097(8) 0.101(11) -0.045(8) -0.036(8) 0.061(7) C3 0.119(11) 0.119(10) 0.132(13) -0.057(10) -0.044(10) 0.082(9) C4 0.110(10) 0.105(10) 0.102(11) -0.061(9) -0.028(9) 0.063(9) C5 0.097(9) 0.087(9) 0.061(8) -0.011(7) -0.006(7) 0.025(7) C6 0.078(7) 0.067(7) 0.081(9) 0.006(7) 0.012(7) 0.039(6) C7 0.109(9) 0.094(8) 0.064(8) -0.013(7) -0.030(7) 0.074(7) C8 0.30(2) 0.130(13) 0.097(13) -0.033(11) -0.053(15) 0.158(15) C9 0.41(3) 0.150(15) 0.106(14) -0.016(13) -0.068(18) 0.21(2) C10 0.33(3) 0.134(15) 0.083(13) 0.009(12) -0.058(15) 0.149(17) C11 0.155(13) 0.106(11) 0.086(12) -0.012(10) -0.031(10) 0.084(10) C12 0.103(9) 0.081(8) 0.069(9) -0.011(7) -0.013(7) 0.059(7) C13 0.082(9) 0.141(12) 0.090(11) -0.044(10) -0.022(8) 0.055(10) C14 0.081(11) 0.146(16) 0.18(2) -0.084(15) 0.003(12) 0.039(11) C15 0.16(2) 0.42(5) 0.14(2) -0.12(3) -0.056(19) 0.19(3) C16 0.120(16) 0.132(15) 0.15(2) -0.087(16) 0.036(15) -0.018(14) C17 0.135(16) 0.30(3) 0.146(19) -0.13(2) -0.073(16) 0.16(2) C18 0.117(12) 0.155(15) 0.089(11) -0.019(10) 0.000(9) 0.099(12) C19 0.073(8) 0.103(9) 0.071(9) 0.009(7) 0.013(7) 0.035(7) C20 0.083(9) 0.080(8) 0.080(9) -0.009(7) 0.000(7) 0.029(8) C21 0.087(11) 0.135(14) 0.133(15) -0.024(12) 0.016(10) 0.032(11) C22 0.122(15) 0.101(13) 0.23(3) -0.010(15) 0.036(16) 0.015(12) C23 0.154(16) 0.063(10) 0.23(2) -0.003(12) 0.022(16) 0.040(11) C24 0.121(12) 0.067(9) 0.179(16) 0.009(10) 0.014(12) 0.052(9) C25 0.105(12) 0.144(16) 0.032(8) 0.000 0.000 0.098(13) C26 0.118(16) 0.18(2) 0.058(12) 0.000 0.000 0.116(17) C27 0.21(3) 0.22(3) 0.062(13) 0.000 0.000 0.19(2) C28 0.33(4) 0.19(3) 0.071(14) 0.000 0.000 0.22(3) C29 0.17(2) 0.115(18) 0.091(16) 0.000 0.000 0.107(18) C30 0.154(19) 0.062(11) 0.086(15) 0.000 0.000 0.060(14) C31 0.121(15) 0.22(2) 0.060(12) 0.000 0.000 0.147(18) C32 0.11(2) 0.22(3) 0.067(14) 0.000 0.000 0.13(2) C33 0.16(3) 0.48(8) 0.058(16) 0.000 0.000 0.19(4) C34 0.60(11) 0.32(5) 0.07(2) 0.000 0.000 0.38(7) C35 0.60(11) 0.55(11) 0.034(15) 0.000 0.000 0.47(11) C36 0.44(7) 0.27(5) 0.040(12) 0.000 0.000 0.33(5) F8 0.415(17) 0.215(10) 0.074(6) -0.040(7) -0.054(9) 0.254(12) F9 0.80(4) 0.224(12) 0.137(10) -0.052(9) -0.117(16) 0.38(2) F10 0.49(2) 0.156(9) 0.131(9) 0.006(8) -0.075(12) 0.198(12) F11 0.196(9) 0.125(6) 0.094(7) 0.013(5) -0.007(6) 0.079(6) F12 0.141(6) 0.103(5) 0.087(6) 0.006(4) 0.032(5) 0.067(5) F14 0.126(6) 0.077(4) 0.127(7) -0.003(5) 0.013(6) 0.021(4) F15 0.218(13) 0.214(14) 0.255(19) -0.074(13) 0.135(13) -0.046(12) F16 0.069(5) 0.373(19) 0.296(18) -0.157(16) -0.010(8) 0.067(9) F17 0.191(11) 0.47(2) 0.230(15) -0.144(15) -0.067(10) 0.249(15) F18 0.214(11) 0.292(14) 0.137(9) -0.046(10) -0.036(8) 0.212(11) F20 0.092(5) 0.135(6) 0.103(6) -0.028(5) 0.004(4) 0.060(5) F21 0.100(6) 0.188(9) 0.192(10) -0.046(8) -0.012(6) 0.046(6) F23 0.240(13) 0.088(6) 0.45(3) -0.037(10) 0.021(14) 0.065(7) F24 0.164(8) 0.106(6) 0.235(12) 0.036(7) 0.030(8) 0.088(6) F26 0.078(6) 0.165(10) 0.085(8) 0.000 0.000 0.078(7) F27 0.210(13) 0.32(2) 0.157(13) 0.000 0.000 0.236(15) F29 0.33(2) 0.088(8) 0.142(13) 0.000 0.000 0.118(11) F30 0.109(8) 0.084(6) 0.104(9) 0.000 0.000 0.044(6) F32 0.068(8) 0.41(3) 0.141(14) 0.000 0.000 0.097(14) F33 0.220(19) 0.68(5) 0.24(2) 0.000 0.000 0.33(3) F35 0.63(5) 0.35(3) 0.129(15) 0.000 0.000 0.43(4) F36 0.29(2) 0.126(10) 0.145(14) 0.000 0.000 0.139(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.268(3) . ? Pt1 S1 2.327(3) . ? Pt1 S2 2.359(2) . ? Pt1 S3 2.370(2) . ? P1 C1 1.798(11) . ? P1 C13 1.817(14) . ? P1 C7 1.839(12) . ? S1 C19 1.770(12) . ? S2 C25 1.829(15) . ? S2 Pt1 2.359(2) 10_556 ? S3 C31 1.769(19) . ? S3 Pt1 2.370(2) 10_556 ? C1 C6 1.364(14) . ? C1 C2 1.387(14) . ? C2 C3 1.373(15) . ? C2 H2A 0.9300 . ? C3 C4 1.342(16) . ? C3 H3A 0.9300 . ? C4 C5 1.328(16) . ? C4 H4A 0.9300 . ? C5 C6 1.398(15) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.347(15) . ? C7 C8 1.375(16) . ? C8 F8 1.350(19) . ? C8 C9 1.36(2) . ? C9 F9 1.365(17) . ? C9 C10 1.37(3) . ? C10 F10 1.289(16) . ? C10 C11 1.34(2) . ? C11 F11 1.317(17) . ? C11 C12 1.386(17) . ? C12 F12 1.349(12) . ? C13 C14 1.383(9) . ? C13 C18 1.400(9) . ? C14 F14 1.351(18) . ? C14 C15 1.409(10) . ? C15 F15 1.26(3) . ? C15 C16 1.369(10) . ? C16 F16 1.34(2) . ? C16 C17 1.373(10) . ? C17 C18 1.377(9) . ? C17 F17 1.390(19) . ? C18 F18 1.347(16) . ? C19 C24 1.376(16) . ? C19 C20 1.410(16) . ? C20 F20 1.346(13) . ? C20 C21 1.357(18) . ? C21 C22 1.30(2) . ? C21 F21 1.402(17) . ? C22 C23 1.37(2) . ? C22 H22A 0.9300 . ? C23 C24 1.36(2) . ? C23 F23 1.366(18) . ? C24 F24 1.356(15) . ? C25 C26 1.394(9) . ? C25 C30 1.399(10) . ? C26 F26 1.363(18) . ? C26 C27 1.397(10) . ? C27 F27 1.38(2) . ? C27 C28 1.390(10) . ? C28 C29 1.384(10) . ? C28 H28A 0.9300 . ? C29 F29 1.29(2) . ? C29 C30 1.386(10) . ? C30 F30 1.276(19) . ? C31 C36 1.387(10) . ? C31 C32 1.397(10) . ? C32 F32 1.30(3) . ? C32 C33 1.383(10) . ? C33 C34 1.378(10) . ? C33 F33 1.42(3) . ? C34 C35 1.381(10) . ? C34 H34A 0.9300 . ? C35 F35 1.33(2) . ? C35 C36 1.389(10) . ? C36 F36 1.26(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 S1 86.44(11) . . ? P1 Pt1 S2 98.65(10) . . ? S1 Pt1 S2 174.71(10) . . ? P1 Pt1 S3 177.94(12) . . ? S1 Pt1 S3 93.83(10) . . ? S2 Pt1 S3 81.13(9) . . ? C1 P1 C13 101.5(6) . . ? C1 P1 C7 105.9(5) . . ? C13 P1 C7 104.4(6) . . ? C1 P1 Pt1 117.3(4) . . ? C13 P1 Pt1 115.6(4) . . ? C7 P1 Pt1 110.9(4) . . ? C19 S1 Pt1 105.8(4) . . ? C25 S2 Pt1 104.1(3) . 10_556 ? C25 S2 Pt1 104.1(3) . . ? Pt1 S2 Pt1 98.71(13) 10_556 . ? C31 S3 Pt1 105.7(5) . . ? C31 S3 Pt1 105.7(5) . 10_556 ? Pt1 S3 Pt1 98.11(13) . 10_556 ? C6 C1 C2 116.0(10) . . ? C6 C1 P1 121.5(8) . . ? C2 C1 P1 122.4(8) . . ? C3 C2 C1 120.8(11) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? C4 C3 C2 121.6(12) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C5 C4 C3 119.2(12) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 120.3(12) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C1 C6 C5 121.8(11) . . ? C1 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C12 C7 C8 113.5(13) . . ? C12 C7 P1 127.8(10) . . ? C8 C7 P1 118.6(11) . . ? F8 C8 C9 118.7(14) . . ? F8 C8 C7 119.0(14) . . ? C9 C8 C7 122.3(17) . . ? F9 C9 C8 117.1(18) . . ? F9 C9 C10 120.2(16) . . ? C8 C9 C10 122.7(16) . . ? F10 C10 C11 125.5(18) . . ? F10 C10 C9 118.4(18) . . ? C11 C10 C9 116.0(16) . . ? F11 C11 C10 117.5(15) . . ? F11 C11 C12 122.0(13) . . ? C10 C11 C12 120.5(16) . . ? C7 C12 F12 121.2(11) . . ? C7 C12 C11 125.0(13) . . ? F12 C12 C11 113.7(12) . . ? C14 C13 C18 113.0(15) . . ? C14 C13 P1 115.2(11) . . ? C18 C13 P1 130.9(14) . . ? F14 C14 C13 119.5(13) . . ? F14 C14 C15 110.2(18) . . ? C13 C14 C15 130(2) . . ? F15 C15 C16 124.2(19) . . ? F15 C15 C14 126(2) . . ? C16 C15 C14 109(2) . . ? F16 C16 C15 124.7(17) . . ? F16 C16 C17 108(2) . . ? C15 C16 C17 127(2) . . ? C16 C17 C18 117.9(17) . . ? C16 C17 F17 128.5(19) . . ? C18 C17 F17 113.2(17) . . ? F18 C18 C17 119.1(14) . . ? F18 C18 C13 117.9(15) . . ? C17 C18 C13 121.7(15) . . ? C24 C19 C20 115.4(12) . . ? C24 C19 S1 126.5(11) . . ? C20 C19 S1 118.1(10) . . ? F20 C20 C21 119.3(14) . . ? F20 C20 C19 120.7(11) . . ? C21 C20 C19 120.0(13) . . ? C22 C21 C20 125.4(17) . . ? C22 C21 F21 117.5(18) . . ? C20 C21 F21 116.6(17) . . ? C21 C22 C23 113.9(19) . . ? C21 C22 H22A 123.0 . . ? C23 C22 H22A 123.0 . . ? C24 C23 C22 125.0(16) . . ? C24 C23 F23 113.2(19) . . ? C22 C23 F23 121.4(19) . . ? F24 C24 C23 122.2(15) . . ? F24 C24 C19 118.0(14) . . ? C23 C24 C19 119.5(15) . . ? C26 C25 C30 123.1(16) . . ? C26 C25 S2 115.5(12) . . ? C30 C25 S2 121.4(10) . . ? F26 C26 C25 122.1(14) . . ? F26 C26 C27 121.5(15) . . ? C25 C26 C27 116.4(17) . . ? F27 C27 C28 123.2(16) . . ? F27 C27 C26 114.5(19) . . ? C28 C27 C26 122.2(19) . . ? C29 C28 C27 119(2) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? F29 C29 C30 122(2) . . ? F29 C29 C28 116.8(17) . . ? C30 C29 C28 121(2) . . ? F30 C30 C29 118.0(16) . . ? F30 C30 C25 124.2(13) . . ? C29 C30 C25 117.8(19) . . ? C36 C31 C32 125(2) . . ? C36 C31 S3 121.1(15) . . ? C32 C31 S3 113.8(18) . . ? F32 C32 C33 115(2) . . ? F32 C32 C31 126(2) . . ? C33 C32 C31 119(2) . . ? C34 C33 C32 121(3) . . ? C34 C33 F33 122(2) . . ? C32 C33 F33 117(2) . . ? C33 C34 C35 114(3) . . ? C33 C34 H34A 123.1 . . ? C35 C34 H34A 123.1 . . ? F35 C35 C34 110(3) . . ? F35 C35 C36 119(3) . . ? C34 C35 C36 132(3) . . ? F36 C36 C31 124(2) . . ? F36 C36 C35 127(3) . . ? C31 C36 C35 109(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Pt1 P1 C1 -59.0(4) . . . . ? S2 Pt1 P1 C1 119.5(4) . . . . ? S3 Pt1 P1 C1 -157(3) . . . . ? S1 Pt1 P1 C13 -178.7(6) . . . . ? S2 Pt1 P1 C13 -0.2(6) . . . . ? S3 Pt1 P1 C13 84(3) . . . . ? S1 Pt1 P1 C7 62.7(4) . . . . ? S2 Pt1 P1 C7 -118.7(4) . . . . ? S3 Pt1 P1 C7 -35(3) . . . . ? P1 Pt1 S1 C19 -139.8(5) . . . . ? S2 Pt1 S1 C19 56.0(14) . . . . ? S3 Pt1 S1 C19 38.2(5) . . . . ? P1 Pt1 S2 C25 78.2(4) . . . . ? S1 Pt1 S2 C25 -117.7(13) . . . . ? S3 Pt1 S2 C25 -99.7(4) . . . . ? P1 Pt1 S2 Pt1 -174.80(12) . . . 10_556 ? S1 Pt1 S2 Pt1 -10.7(13) . . . 10_556 ? S3 Pt1 S2 Pt1 7.28(13) . . . 10_556 ? P1 Pt1 S3 C31 160(3) . . . . ? S1 Pt1 S3 C31 62.2(6) . . . . ? S2 Pt1 S3 C31 -116.1(6) . . . . ? P1 Pt1 S3 Pt1 -91(3) . . . 10_556 ? S1 Pt1 S3 Pt1 171.13(13) . . . 10_556 ? S2 Pt1 S3 Pt1 -7.24(13) . . . 10_556 ? C13 P1 C1 C6 -40.8(11) . . . . ? C7 P1 C1 C6 67.9(10) . . . . ? Pt1 P1 C1 C6 -167.7(8) . . . . ? C13 P1 C1 C2 139.5(11) . . . . ? C7 P1 C1 C2 -111.8(10) . . . . ? Pt1 P1 C1 C2 12.6(12) . . . . ? C6 C1 C2 C3 0.1(19) . . . . ? P1 C1 C2 C3 179.8(11) . . . . ? C1 C2 C3 C4 -4(2) . . . . ? C2 C3 C4 C5 6(2) . . . . ? C3 C4 C5 C6 -3(2) . . . . ? C2 C1 C6 C5 2.0(16) . . . . ? P1 C1 C6 C5 -177.7(9) . . . . ? C4 C5 C6 C1 -0.4(19) . . . . ? C1 P1 C7 C12 7.1(13) . . . . ? C13 P1 C7 C12 113.7(12) . . . . ? Pt1 P1 C7 C12 -121.1(11) . . . . ? C1 P1 C7 C8 -176.4(12) . . . . ? C13 P1 C7 C8 -69.8(13) . . . . ? Pt1 P1 C7 C8 55.4(13) . . . . ? C12 C7 C8 F8 177.9(16) . . . . ? P1 C7 C8 F8 1(2) . . . . ? C12 C7 C8 C9 1(3) . . . . ? P1 C7 C8 C9 -176.4(17) . . . . ? F8 C8 C9 F9 3(3) . . . . ? C7 C8 C9 F9 -179.3(19) . . . . ? F8 C8 C9 C10 -178(2) . . . . ? C7 C8 C9 C10 0(4) . . . . ? F9 C9 C10 F10 3(4) . . . . ? C8 C9 C10 F10 -176(2) . . . . ? F9 C9 C10 C11 179.1(19) . . . . ? C8 C9 C10 C11 0(4) . . . . ? F10 C10 C11 F11 -3(3) . . . . ? C9 C10 C11 F11 -179(2) . . . . ? F10 C10 C11 C12 175.9(19) . . . . ? C9 C10 C11 C12 0(3) . . . . ? C8 C7 C12 F12 -177.2(13) . . . . ? P1 C7 C12 F12 -0.5(18) . . . . ? C8 C7 C12 C11 -1(2) . . . . ? P1 C7 C12 C11 175.9(10) . . . . ? F11 C11 C12 C7 179.7(13) . . . . ? C10 C11 C12 C7 1(2) . . . . ? F11 C11 C12 F12 -4(2) . . . . ? C10 C11 C12 F12 177.3(16) . . . . ? C1 P1 C13 C14 -58.1(10) . . . . ? C7 P1 C13 C14 -168.0(9) . . . . ? Pt1 P1 C13 C14 70.0(10) . . . . ? C1 P1 C13 C18 109.7(13) . . . . ? C7 P1 C13 C18 -0.2(15) . . . . ? Pt1 P1 C13 C18 -122.3(12) . . . . ? C18 C13 C14 F14 -176.5(13) . . . . ? P1 C13 C14 F14 -6.5(15) . . . . ? C18 C13 C14 C15 2.4(15) . . . . ? P1 C13 C14 C15 172.4(11) . . . . ? F14 C14 C15 F15 -5(2) . . . . ? C13 C14 C15 F15 176(2) . . . . ? F14 C14 C15 C16 -179.2(17) . . . . ? C13 C14 C15 C16 1.8(17) . . . . ? F15 C15 C16 F16 5(4) . . . . ? C14 C15 C16 F16 179.0(15) . . . . ? F15 C15 C16 C17 -174(2) . . . . ? C14 C15 C16 C17 1(3) . . . . ? F16 C16 C17 C18 174.4(13) . . . . ? C15 C16 C17 C18 -7(3) . . . . ? F16 C16 C17 F17 3(3) . . . . ? C15 C16 C17 F17 -178.7(17) . . . . ? C16 C17 C18 F18 178.3(16) . . . . ? F17 C17 C18 F18 -9(2) . . . . ? C16 C17 C18 C13 12(2) . . . . ? F17 C17 C18 C13 -175.5(13) . . . . ? C14 C13 C18 F18 -176.1(13) . . . . ? P1 C13 C18 F18 16(2) . . . . ? C14 C13 C18 C17 -9(2) . . . . ? P1 C13 C18 C17 -177.2(12) . . . . ? Pt1 S1 C19 C24 52.3(14) . . . . ? Pt1 S1 C19 C20 -126.6(10) . . . . ? C24 C19 C20 F20 -177.2(12) . . . . ? S1 C19 C20 F20 1.8(17) . . . . ? C24 C19 C20 C21 4(2) . . . . ? S1 C19 C20 C21 -176.7(12) . . . . ? F20 C20 C21 C22 174.9(19) . . . . ? C19 C20 C21 C22 -7(3) . . . . ? F20 C20 C21 F21 3(2) . . . . ? C19 C20 C21 F21 -178.3(13) . . . . ? C20 C21 C22 C23 8(3) . . . . ? F21 C21 C22 C23 179.9(18) . . . . ? C21 C22 C23 C24 -9(4) . . . . ? C21 C22 C23 F23 178.8(19) . . . . ? C22 C23 C24 F24 -179(2) . . . . ? F23 C23 C24 F24 -6(3) . . . . ? C22 C23 C24 C19 8(3) . . . . ? F23 C23 C24 C19 -179.5(16) . . . . ? C20 C19 C24 F24 -178.5(13) . . . . ? S1 C19 C24 F24 3(2) . . . . ? C20 C19 C24 C23 -5(2) . . . . ? S1 C19 C24 C23 176.3(14) . . . . ? Pt1 S2 C25 C26 128.54(13) 10_556 . . . ? Pt1 S2 C25 C26 -128.54(13) . . . . ? Pt1 S2 C25 C30 -51.46(13) 10_556 . . . ? Pt1 S2 C25 C30 51.46(13) . . . . ? C30 C25 C26 F26 180.0 . . . . ? S2 C25 C26 F26 0.0 . . . . ? C30 C25 C26 C27 0.0 . . . . ? S2 C25 C26 C27 180.0 . . . . ? F26 C26 C27 F27 0.0 . . . . ? C25 C26 C27 F27 180.0 . . . . ? F26 C26 C27 C28 180.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? F27 C27 C28 C29 180.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 F29 180.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? F29 C29 C30 F30 0.0 . . . . ? C28 C29 C30 F30 180.0 . . . . ? F29 C29 C30 C25 180.0 . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 F30 180.0 . . . . ? S2 C25 C30 F30 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? S2 C25 C30 C29 180.0 . . . . ? Pt1 S3 C31 C36 51.69(19) . . . . ? Pt1 S3 C31 C36 -51.7(2) 10_556 . . . ? Pt1 S3 C31 C32 -128.31(19) . . . . ? Pt1 S3 C31 C32 128.31(19) 10_556 . . . ? C36 C31 C32 F32 180.0 . . . . ? S3 C31 C32 F32 0.0 . . . . ? C36 C31 C32 C33 0.0 . . . . ? S3 C31 C32 C33 180.0 . . . . ? F32 C32 C33 C34 180.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? F32 C32 C33 F33 0.0 . . . . ? C31 C32 C33 F33 180.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? F33 C33 C34 C35 180.0 . . . . ? C33 C34 C35 F35 180.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C32 C31 C36 F36 180.0 . . . . ? S3 C31 C36 F36 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? S3 C31 C36 C35 180.0 . . . . ? F35 C35 C36 F36 0.0 . . . . ? C34 C35 C36 F36 180.0 . . . . ? F35 C35 C36 C31 180.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.741 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.119 ######################################################## # End of Crystallographic Information File (CIF) # ######################################################## data_lv34 _database_code_depnum_ccdc_archive 'CCDC 239572' _audit_creation_method SHELXL-97 _audit_creation_date 2003-06-02 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H13 F16 P Pt S3' _chemical_formula_sum 'C36 H13 F16 P Pt S3' _chemical_formula_weight 1071.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.945(3) _cell_length_b 12.0754(14) _cell_length_c 13.4898(18) _cell_angle_alpha 102.108(10) _cell_angle_beta 102.397(17) _cell_angle_gamma 105.499(14) _cell_volume 1755.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 11.93 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 4.334 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.449 _exptl_absorpt_correction_T_max 0.531 _exptl_absorpt_process_details '23 psi scans with XSCAnS 2.21 (Fait, 1996)' _exptl_special_details ? _diffrn_ambient_temperature 293(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_source_power 1.5 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_detector 'Scintillation counter' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.92 _diffrn_reflns_number 7081 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6109 _reflns_number_gt 4627 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'XSCAnS 2.21 (Fait, 1996)' _computing_cell_refinement 'XSCAnS 2.21 (Fait, 1996)' _computing_data_reduction 'XSCAnS 2.21 (Fait, 1996)' _computing_structure_solution 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.1215P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6109 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.14597(3) 0.20705(3) 0.22256(3) 0.03911(12) Uani 1 1 d . . . P1 P 0.26666(19) 0.1410(2) 0.33257(17) 0.0411(5) Uani 1 1 d . . . S1 S 0.1818(2) 0.0971(2) 0.08183(17) 0.0482(5) Uani 1 1 d . . . S2 S 0.1194(2) 0.3263(2) 0.36670(17) 0.0519(6) Uani 1 1 d . . . S3 S 0.0104(2) 0.2475(2) 0.08881(18) 0.0557(6) Uani 1 1 d . . . C1 C 0.2914(8) 0.0349(7) 0.1392(7) 0.050(2) Uani 1 1 d . . . C2 C 0.3314(7) 0.0533(7) 0.2484(6) 0.044(2) Uani 1 1 d . . . C3 C 0.4146(8) -0.0002(8) 0.2827(8) 0.058(2) Uani 1 1 d . . . F3 F 0.4589(6) 0.0136(6) 0.3862(5) 0.0834(18) Uani 1 1 d . . . C4 C 0.4571(9) -0.0682(9) 0.2156(10) 0.073(3) Uani 1 1 d . . . F4 F 0.5421(6) -0.1148(7) 0.2517(6) 0.105(2) Uani 1 1 d . . . C5 C 0.4170(10) -0.0850(9) 0.1063(9) 0.072(3) Uani 1 1 d . . . F5 F 0.4618(7) -0.1478(7) 0.0382(6) 0.108(2) Uani 1 1 d . . . C6 C 0.3323(9) -0.0341(8) 0.0685(8) 0.058(3) Uani 1 1 d . . . F6 F 0.2939(5) -0.0509(5) -0.0360(4) 0.0764(16) Uani 1 1 d . . . C7 C 0.2759(8) 0.1960(8) 0.0286(6) 0.050(2) Uani 1 1 d . . . C8 C 0.3871(8) 0.2806(8) 0.0886(7) 0.056(2) Uani 1 1 d . . . F8 F 0.4251(5) 0.2976(5) 0.1921(4) 0.0671(15) Uani 1 1 d . . . C9 C 0.4579(11) 0.3460(10) 0.0383(10) 0.076(3) Uani 1 1 d . . . F9 F 0.5664(7) 0.4257(7) 0.1002(7) 0.119(3) Uani 1 1 d . . . C10 C 0.4220(14) 0.3329(12) -0.0681(11) 0.090(4) Uani 1 1 d . . . H10A H 0.4717 0.3773 -0.1002 0.108 Uiso 1 1 calc R . . C11 C 0.3127(14) 0.2541(13) -0.1245(9) 0.083(4) Uani 1 1 d . . . F11 F 0.2742(8) 0.2374(8) -0.2298(5) 0.125(3) Uani 1 1 d . . . C12 C 0.2395(11) 0.1827(11) -0.0807(8) 0.073(3) Uani 1 1 d . . . F12 F 0.1338(7) 0.1040(6) -0.1386(4) 0.098(2) Uani 1 1 d . . . C13 C 0.1917(8) 0.0345(8) 0.3950(6) 0.049(2) Uani 1 1 d . . . C14 C 0.0706(9) -0.0252(9) 0.3515(7) 0.066(3) Uani 1 1 d . . . H14A H 0.0266 -0.0078 0.2945 0.080 Uiso 1 1 calc R . . C15 C 0.0136(11) -0.1135(10) 0.3946(10) 0.089(4) Uani 1 1 d . . . H15A H -0.0690 -0.1548 0.3657 0.107 Uiso 1 1 calc R . . C16 C 0.0754(11) -0.1386(11) 0.4751(10) 0.093(4) Uani 1 1 d . . . H16A H 0.0372 -0.1996 0.5008 0.111 Uiso 1 1 calc R . . C17 C 0.1946(12) -0.0758(12) 0.5207(10) 0.095(4) Uani 1 1 d . . . H17A H 0.2369 -0.0922 0.5792 0.114 Uiso 1 1 calc R . . C18 C 0.2538(10) 0.0115(10) 0.4820(8) 0.081(3) Uani 1 1 d . . . H18A H 0.3355 0.0549 0.5145 0.097 Uiso 1 1 calc R . . C19 C 0.3934(7) 0.2514(7) 0.4382(6) 0.045(2) Uani 1 1 d . . . C20 C 0.5085(8) 0.2896(8) 0.4277(7) 0.057(2) Uani 1 1 d . . . H20A H 0.5250 0.2553 0.3663 0.069 Uiso 1 1 calc R . . C21 C 0.5996(9) 0.3792(10) 0.5087(8) 0.078(3) Uani 1 1 d . . . H21A H 0.6777 0.4042 0.5022 0.093 Uiso 1 1 calc R . . C22 C 0.5763(10) 0.4290(11) 0.5949(9) 0.083(4) Uani 1 1 d . . . H22A H 0.6381 0.4905 0.6479 0.100 Uiso 1 1 calc R . . C23 C 0.4612(11) 0.3922(10) 0.6091(8) 0.074(3) Uani 1 1 d . . . H23A H 0.4469 0.4271 0.6715 0.089 Uiso 1 1 calc R . . C24 C 0.3696(9) 0.3039(9) 0.5300(7) 0.063(3) Uani 1 1 d . . . H24A H 0.2919 0.2791 0.5376 0.076 Uiso 1 1 calc R . . C25 C -0.0250(7) 0.3448(8) 0.3319(6) 0.042(2) Uani 1 1 d . . . C26 C -0.0340(8) 0.4583(8) 0.3574(6) 0.048(2) Uani 1 1 d . . . F26 F 0.0672(5) 0.5549(5) 0.3992(4) 0.0705(15) Uani 1 1 d . . . C27 C -0.1435(10) 0.4768(9) 0.3390(8) 0.058(2) Uani 1 1 d . . . F27 F -0.1475(6) 0.5892(5) 0.3623(5) 0.0885(19) Uani 1 1 d . . . C28 C -0.2487(9) 0.3850(10) 0.2969(8) 0.065(3) Uani 1 1 d . . . H28A H -0.3231 0.3981 0.2839 0.078 Uiso 1 1 calc R . . C29 C -0.2416(8) 0.2725(9) 0.2742(7) 0.058(2) Uani 1 1 d . . . F29 F -0.3446(5) 0.1738(6) 0.2319(5) 0.090(2) Uani 1 1 d . . . C30 C -0.1332(8) 0.2498(8) 0.2903(7) 0.050(2) Uani 1 1 d . . . F30 F -0.1314(5) 0.1373(5) 0.2664(4) 0.0666(15) Uani 1 1 d . . . C31 C 0.0402(10) 0.4039(9) 0.1187(7) 0.059(3) Uani 1 1 d . . . C32 C 0.1555(11) 0.4872(10) 0.1494(8) 0.070(3) Uani 1 1 d . . . F32 F 0.2522(5) 0.4510(5) 0.1532(5) 0.0821(17) Uani 1 1 d . . . C33 C 0.1739(17) 0.6106(12) 0.1718(10) 0.102(5) Uani 1 1 d . . . F33 F 0.2878(11) 0.6840(7) 0.1976(7) 0.153(4) Uani 1 1 d . . . C34 C 0.084(2) 0.6541(16) 0.1645(12) 0.131(7) Uani 1 1 d . . . H34B H 0.0983 0.7363 0.1799 0.158 Uiso 1 1 calc R . . C35 C -0.034(2) 0.5731(18) 0.1329(12) 0.117(6) Uani 1 1 d . . . F35 F -0.1345(10) 0.6061(10) 0.1213(8) 0.172(5) Uani 1 1 d . . . C36 C -0.0544(13) 0.4501(13) 0.1102(9) 0.086(4) Uani 1 1 d . . . F36 F -0.1696(8) 0.3736(9) 0.0769(6) 0.114(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03234(17) 0.04245(19) 0.04046(18) 0.01202(13) 0.00540(12) 0.01274(13) P1 0.0332(11) 0.0459(13) 0.0420(12) 0.0155(10) 0.0050(9) 0.0114(10) S1 0.0402(12) 0.0551(14) 0.0417(12) 0.0052(10) 0.0017(10) 0.0179(11) S2 0.0450(13) 0.0634(15) 0.0442(12) 0.0082(11) 0.0072(10) 0.0224(12) S3 0.0514(14) 0.0674(16) 0.0487(13) 0.0175(11) 0.0016(11) 0.0294(12) C1 0.040(5) 0.038(5) 0.067(6) 0.009(4) 0.010(5) 0.014(4) C2 0.039(5) 0.037(4) 0.051(5) 0.015(4) 0.003(4) 0.009(4) C3 0.049(6) 0.052(6) 0.073(7) 0.023(5) 0.006(5) 0.020(5) F3 0.083(4) 0.098(5) 0.074(4) 0.030(3) 0.001(3) 0.051(4) C4 0.063(7) 0.066(7) 0.102(9) 0.024(6) 0.018(6) 0.045(6) F4 0.091(5) 0.118(6) 0.127(6) 0.036(5) 0.021(4) 0.077(5) C5 0.072(7) 0.067(7) 0.082(8) 0.007(6) 0.023(6) 0.043(6) F5 0.110(6) 0.118(6) 0.108(5) 0.007(4) 0.035(4) 0.073(5) C6 0.055(6) 0.057(6) 0.061(6) 0.012(5) 0.010(5) 0.025(5) F6 0.084(4) 0.076(4) 0.064(4) 0.000(3) 0.019(3) 0.036(3) C7 0.050(5) 0.068(6) 0.039(5) 0.019(4) 0.013(4) 0.030(5) C8 0.050(6) 0.058(6) 0.061(6) 0.017(5) 0.018(5) 0.017(5) F8 0.057(3) 0.075(4) 0.051(3) 0.020(3) -0.002(3) 0.005(3) C9 0.073(8) 0.076(8) 0.086(8) 0.036(7) 0.021(7) 0.025(7) F9 0.093(5) 0.104(6) 0.150(7) 0.068(5) 0.028(5) -0.003(5) C10 0.114(11) 0.096(10) 0.108(11) 0.067(8) 0.058(9) 0.058(9) C11 0.116(11) 0.118(11) 0.069(8) 0.058(8) 0.055(8) 0.077(9) F11 0.173(8) 0.189(8) 0.063(4) 0.069(5) 0.047(5) 0.102(7) C12 0.079(8) 0.090(8) 0.055(6) 0.012(6) 0.006(6) 0.054(7) F12 0.107(5) 0.117(5) 0.046(3) 0.006(3) -0.012(4) 0.037(5) C13 0.051(5) 0.050(5) 0.047(5) 0.022(4) 0.012(4) 0.016(4) C14 0.054(6) 0.070(7) 0.058(6) 0.021(5) -0.003(5) 0.004(5) C15 0.070(8) 0.074(8) 0.095(9) 0.029(7) 0.010(7) -0.013(6) C16 0.080(9) 0.081(8) 0.107(10) 0.058(8) 0.014(8) -0.005(7) C17 0.094(10) 0.113(10) 0.089(9) 0.072(8) 0.019(8) 0.026(8) C18 0.060(7) 0.098(8) 0.083(7) 0.061(7) 0.007(6) 0.006(6) C19 0.041(5) 0.048(5) 0.043(5) 0.014(4) 0.007(4) 0.014(4) C20 0.042(5) 0.071(6) 0.052(5) 0.023(5) 0.007(4) 0.008(5) C21 0.049(6) 0.093(8) 0.056(7) 0.020(6) -0.005(5) -0.015(6) C22 0.060(8) 0.090(9) 0.062(7) 0.016(6) -0.018(6) -0.003(6) C23 0.081(8) 0.080(8) 0.045(6) 0.002(5) 0.004(6) 0.025(7) C24 0.051(6) 0.069(7) 0.057(6) 0.011(5) 0.002(5) 0.016(5) C25 0.040(5) 0.055(6) 0.036(4) 0.014(4) 0.014(4) 0.018(4) C26 0.055(6) 0.050(6) 0.038(5) 0.012(4) 0.012(4) 0.013(5) F26 0.067(4) 0.054(3) 0.077(4) 0.009(3) 0.013(3) 0.013(3) C27 0.070(7) 0.057(6) 0.063(6) 0.020(5) 0.032(6) 0.034(6) F27 0.104(5) 0.071(4) 0.110(5) 0.023(4) 0.041(4) 0.054(4) C28 0.054(6) 0.086(8) 0.070(7) 0.028(6) 0.021(5) 0.040(6) C29 0.040(5) 0.071(7) 0.054(6) 0.008(5) 0.017(4) 0.008(5) F29 0.042(3) 0.100(5) 0.111(5) 0.011(4) 0.026(3) 0.005(3) C30 0.053(6) 0.050(5) 0.054(5) 0.021(4) 0.021(5) 0.019(5) F30 0.065(4) 0.050(3) 0.080(4) 0.012(3) 0.023(3) 0.014(3) C31 0.083(7) 0.077(7) 0.045(5) 0.032(5) 0.027(5) 0.054(6) C32 0.093(9) 0.066(7) 0.062(6) 0.024(5) 0.023(6) 0.041(7) F32 0.071(4) 0.066(4) 0.094(4) 0.020(3) 0.003(3) 0.017(3) C33 0.159(15) 0.071(9) 0.081(9) 0.036(7) 0.021(9) 0.046(11) F33 0.190(10) 0.072(5) 0.149(8) 0.040(5) -0.005(7) 0.002(6) C34 0.26(3) 0.106(13) 0.090(11) 0.058(10) 0.072(15) 0.116(16) C35 0.209(19) 0.153(16) 0.095(11) 0.080(11) 0.087(13) 0.158(15) F35 0.272(12) 0.230(10) 0.172(8) 0.130(8) 0.137(9) 0.219(10) C36 0.112(11) 0.129(11) 0.072(7) 0.063(8) 0.050(8) 0.081(10) F36 0.110(6) 0.196(9) 0.119(6) 0.099(6) 0.067(5) 0.115(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.261(2) . ? Pt1 S1 2.268(2) . ? Pt1 S2 2.300(2) . ? Pt1 S3 2.378(2) . ? P1 C19 1.816(8) . ? P1 C13 1.824(8) . ? P1 C2 1.822(9) . ? S1 C7 1.787(9) . ? S1 C1 1.792(9) . ? S2 C25 1.775(8) . ? S3 C31 1.765(10) . ? C1 C6 1.388(12) . ? C1 C2 1.397(12) . ? C2 C3 1.374(11) . ? C3 F3 1.340(11) . ? C3 C4 1.364(14) . ? C4 F4 1.339(11) . ? C4 C5 1.401(15) . ? C5 F5 1.357(11) . ? C5 C6 1.380(13) . ? C6 F6 1.337(10) . ? C7 C8 1.389(12) . ? C7 C12 1.406(13) . ? C8 F8 1.325(10) . ? C8 C9 1.384(14) . ? C9 C10 1.369(16) . ? C9 F9 1.354(12) . ? C10 C11 1.339(17) . ? C11 F11 1.349(12) . ? C11 C12 1.374(16) . ? C12 F12 1.316(12) . ? C13 C14 1.363(12) . ? C13 C18 1.370(12) . ? C14 C15 1.409(14) . ? C15 C16 1.315(15) . ? C16 C17 1.353(15) . ? C17 C18 1.370(14) . ? C19 C20 1.376(12) . ? C19 C24 1.392(12) . ? C20 C21 1.383(13) . ? C21 C22 1.315(15) . ? C22 C23 1.395(15) . ? C23 C24 1.367(13) . ? C25 C26 1.381(12) . ? C25 C30 1.388(12) . ? C26 F26 1.348(10) . ? C26 C27 1.365(13) . ? C27 F27 1.343(11) . ? C27 C28 1.347(13) . ? C28 C29 1.358(13) . ? C29 F29 1.375(10) . ? C29 C30 1.375(13) . ? C30 F30 1.336(10) . ? C31 C36 1.383(14) . ? C31 C32 1.385(14) . ? C32 F32 1.336(12) . ? C32 C33 1.403(16) . ? C33 C34 1.31(2) . ? C33 F33 1.334(17) . ? C34 C35 1.40(2) . ? C35 F35 1.346(16) . ? C35 C36 1.39(2) . ? C36 F36 1.352(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 S1 89.91(8) . . ? P1 Pt1 S2 89.64(8) . . ? S1 Pt1 S2 176.91(9) . . ? P1 Pt1 S3 171.40(8) . . ? S1 Pt1 S3 83.06(8) . . ? S2 Pt1 S3 97.65(8) . . ? C19 P1 C13 105.5(4) . . ? C19 P1 C2 106.5(4) . . ? C13 P1 C2 103.1(4) . . ? C19 P1 Pt1 118.2(3) . . ? C13 P1 Pt1 116.8(3) . . ? C2 P1 Pt1 105.4(3) . . ? C7 S1 C1 98.4(4) . . ? C7 S1 Pt1 109.0(3) . . ? C1 S1 Pt1 104.5(3) . . ? C25 S2 Pt1 109.7(3) . . ? C31 S3 Pt1 108.6(3) . . ? C6 C1 C2 122.2(8) . . ? C6 C1 S1 115.9(7) . . ? C2 C1 S1 121.8(7) . . ? C3 C2 C1 116.4(8) . . ? C3 C2 P1 125.6(7) . . ? C1 C2 P1 118.1(6) . . ? F3 C3 C4 116.5(8) . . ? F3 C3 C2 120.5(9) . . ? C4 C3 C2 123.1(9) . . ? F4 C4 C3 121.7(10) . . ? F4 C4 C5 118.3(10) . . ? C3 C4 C5 119.9(9) . . ? F5 C5 C6 119.9(10) . . ? F5 C5 C4 121.2(9) . . ? C6 C5 C4 118.8(9) . . ? F6 C6 C5 118.5(9) . . ? F6 C6 C1 121.9(8) . . ? C5 C6 C1 119.5(9) . . ? C8 C7 C12 118.1(9) . . ? C8 C7 S1 123.2(7) . . ? C12 C7 S1 118.5(8) . . ? F8 C8 C9 120.6(9) . . ? F8 C8 C7 120.6(8) . . ? C9 C8 C7 118.8(9) . . ? C10 C9 F9 120.7(11) . . ? C10 C9 C8 122.8(12) . . ? F9 C9 C8 116.5(10) . . ? C11 C10 C9 117.8(12) . . ? C10 C11 F11 119.7(12) . . ? C10 C11 C12 122.6(11) . . ? F11 C11 C12 117.5(13) . . ? F12 C12 C11 121.3(11) . . ? F12 C12 C7 118.9(11) . . ? C11 C12 C7 119.7(11) . . ? C14 C13 C18 119.7(9) . . ? C14 C13 P1 118.2(7) . . ? C18 C13 P1 122.1(7) . . ? C13 C14 C15 118.6(9) . . ? C16 C15 C14 121.0(11) . . ? C15 C16 C17 120.0(10) . . ? C16 C17 C18 121.0(11) . . ? C13 C18 C17 119.4(10) . . ? C20 C19 C24 119.7(8) . . ? C20 C19 P1 122.6(7) . . ? C24 C19 P1 117.6(7) . . ? C19 C20 C21 119.8(10) . . ? C22 C21 C20 120.3(11) . . ? C21 C22 C23 121.8(10) . . ? C24 C23 C22 119.0(10) . . ? C23 C24 C19 119.5(10) . . ? C26 C25 C30 116.6(8) . . ? C26 C25 S2 119.4(7) . . ? C30 C25 S2 123.6(7) . . ? F26 C26 C27 118.1(9) . . ? F26 C26 C25 120.0(8) . . ? C27 C26 C25 121.8(9) . . ? F27 C27 C28 118.7(9) . . ? F27 C27 C26 119.6(10) . . ? C28 C27 C26 121.7(9) . . ? C27 C28 C29 117.3(9) . . ? C28 C29 F29 121.0(9) . . ? C28 C29 C30 123.0(9) . . ? F29 C29 C30 116.0(9) . . ? F30 C30 C29 120.6(8) . . ? F30 C30 C25 119.8(8) . . ? C29 C30 C25 119.6(9) . . ? C36 C31 C32 115.8(11) . . ? C36 C31 S3 120.2(10) . . ? C32 C31 S3 124.0(7) . . ? F32 C32 C31 120.2(9) . . ? F32 C32 C33 118.1(13) . . ? C31 C32 C33 121.6(12) . . ? C34 C33 F33 120.2(15) . . ? C34 C33 C32 122.4(17) . . ? F33 C33 C32 117.4(15) . . ? C33 C34 C35 118.0(16) . . ? F35 C35 C36 115.8(19) . . ? F35 C35 C34 123.8(17) . . ? C36 C35 C34 120.3(14) . . ? F36 C36 C35 119.2(13) . . ? F36 C36 C31 118.9(12) . . ? C35 C36 C31 121.8(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Pt1 P1 C19 124.0(3) . . . . ? S2 Pt1 P1 C19 -52.9(3) . . . . ? S3 Pt1 P1 C19 159.0(6) . . . . ? S1 Pt1 P1 C13 -108.4(3) . . . . ? S2 Pt1 P1 C13 74.6(3) . . . . ? S3 Pt1 P1 C13 -73.4(7) . . . . ? S1 Pt1 P1 C2 5.2(3) . . . . ? S2 Pt1 P1 C2 -171.7(3) . . . . ? S3 Pt1 P1 C2 40.2(7) . . . . ? P1 Pt1 S1 C7 -109.1(3) . . . . ? S2 Pt1 S1 C7 -27.6(17) . . . . ? S3 Pt1 S1 C7 75.9(3) . . . . ? P1 Pt1 S1 C1 -4.7(3) . . . . ? S2 Pt1 S1 C1 76.8(17) . . . . ? S3 Pt1 S1 C1 -179.8(3) . . . . ? P1 Pt1 S2 C25 -150.2(3) . . . . ? S1 Pt1 S2 C25 128.3(16) . . . . ? S3 Pt1 S2 C25 25.2(3) . . . . ? P1 Pt1 S3 C31 -164.7(6) . . . . ? S1 Pt1 S3 C31 -129.4(4) . . . . ? S2 Pt1 S3 C31 47.5(4) . . . . ? C7 S1 C1 C6 -65.6(8) . . . . ? Pt1 S1 C1 C6 -177.9(6) . . . . ? C7 S1 C1 C2 115.4(7) . . . . ? Pt1 S1 C1 C2 3.2(8) . . . . ? C6 C1 C2 C3 0.5(13) . . . . ? S1 C1 C2 C3 179.3(6) . . . . ? C6 C1 C2 P1 -177.7(7) . . . . ? S1 C1 C2 P1 1.1(10) . . . . ? C19 P1 C2 C3 50.8(8) . . . . ? C13 P1 C2 C3 -60.0(8) . . . . ? Pt1 P1 C2 C3 177.1(7) . . . . ? C19 P1 C2 C1 -131.2(7) . . . . ? C13 P1 C2 C1 118.0(7) . . . . ? Pt1 P1 C2 C1 -4.9(7) . . . . ? C1 C2 C3 F3 179.3(8) . . . . ? P1 C2 C3 F3 -2.6(13) . . . . ? C1 C2 C3 C4 -0.3(14) . . . . ? P1 C2 C3 C4 177.8(8) . . . . ? F3 C3 C4 F4 -2.6(15) . . . . ? C2 C3 C4 F4 177.0(9) . . . . ? F3 C3 C4 C5 -178.8(9) . . . . ? C2 C3 C4 C5 0.8(16) . . . . ? F4 C4 C5 F5 0.7(17) . . . . ? C3 C4 C5 F5 177.0(10) . . . . ? F4 C4 C5 C6 -177.9(9) . . . . ? C3 C4 C5 C6 -1.5(17) . . . . ? F5 C5 C6 F6 1.8(15) . . . . ? C4 C5 C6 F6 -179.7(9) . . . . ? F5 C5 C6 C1 -176.8(9) . . . . ? C4 C5 C6 C1 1.7(16) . . . . ? C2 C1 C6 F6 -179.8(8) . . . . ? S1 C1 C6 F6 1.3(12) . . . . ? C2 C1 C6 C5 -1.2(14) . . . . ? S1 C1 C6 C5 179.9(8) . . . . ? C1 S1 C7 C8 -53.7(8) . . . . ? Pt1 S1 C7 C8 54.8(8) . . . . ? C1 S1 C7 C12 122.1(8) . . . . ? Pt1 S1 C7 C12 -129.3(7) . . . . ? C12 C7 C8 F8 179.3(8) . . . . ? S1 C7 C8 F8 -4.8(13) . . . . ? C12 C7 C8 C9 -1.4(14) . . . . ? S1 C7 C8 C9 174.5(8) . . . . ? F8 C8 C9 C10 -179.1(10) . . . . ? C7 C8 C9 C10 1.6(17) . . . . ? F8 C8 C9 F9 0.5(15) . . . . ? C7 C8 C9 F9 -178.8(9) . . . . ? F9 C9 C10 C11 -178.8(11) . . . . ? C8 C9 C10 C11 0.8(18) . . . . ? C9 C10 C11 F11 -179.3(10) . . . . ? C9 C10 C11 C12 -3.4(19) . . . . ? C10 C11 C12 F12 -178.3(11) . . . . ? F11 C11 C12 F12 -2.4(16) . . . . ? C10 C11 C12 C7 3.6(17) . . . . ? F11 C11 C12 C7 179.6(9) . . . . ? C8 C7 C12 F12 -179.2(8) . . . . ? S1 C7 C12 F12 4.7(12) . . . . ? C8 C7 C12 C11 -1.1(14) . . . . ? S1 C7 C12 C11 -177.2(8) . . . . ? C19 P1 C13 C14 152.0(8) . . . . ? C2 P1 C13 C14 -96.5(8) . . . . ? Pt1 P1 C13 C14 18.5(9) . . . . ? C19 P1 C13 C18 -29.4(10) . . . . ? C2 P1 C13 C18 82.1(9) . . . . ? Pt1 P1 C13 C18 -162.9(8) . . . . ? C18 C13 C14 C15 -3.0(16) . . . . ? P1 C13 C14 C15 175.7(9) . . . . ? C13 C14 C15 C16 -0.1(19) . . . . ? C14 C15 C16 C17 3(2) . . . . ? C15 C16 C17 C18 -2(2) . . . . ? C14 C13 C18 C17 3.5(17) . . . . ? P1 C13 C18 C17 -175.1(10) . . . . ? C16 C17 C18 C13 -1(2) . . . . ? C13 P1 C19 C20 133.1(8) . . . . ? C2 P1 C19 C20 24.1(8) . . . . ? Pt1 P1 C19 C20 -94.1(7) . . . . ? C13 P1 C19 C24 -51.0(8) . . . . ? C2 P1 C19 C24 -160.1(7) . . . . ? Pt1 P1 C19 C24 81.7(7) . . . . ? C24 C19 C20 C21 0.4(14) . . . . ? P1 C19 C20 C21 176.2(8) . . . . ? C19 C20 C21 C22 -1.0(16) . . . . ? C20 C21 C22 C23 1.6(18) . . . . ? C21 C22 C23 C24 -1.7(18) . . . . ? C22 C23 C24 C19 1.1(15) . . . . ? C20 C19 C24 C23 -0.5(14) . . . . ? P1 C19 C24 C23 -176.5(8) . . . . ? Pt1 S2 C25 C26 -131.2(6) . . . . ? Pt1 S2 C25 C30 56.3(7) . . . . ? C30 C25 C26 F26 179.3(7) . . . . ? S2 C25 C26 F26 6.3(11) . . . . ? C30 C25 C26 C27 -2.5(12) . . . . ? S2 C25 C26 C27 -175.5(7) . . . . ? F26 C26 C27 F27 0.3(13) . . . . ? C25 C26 C27 F27 -178.0(8) . . . . ? F26 C26 C27 C28 179.6(8) . . . . ? C25 C26 C27 C28 1.4(14) . . . . ? F27 C27 C28 C29 180.0(8) . . . . ? C26 C27 C28 C29 0.6(15) . . . . ? C27 C28 C29 F29 179.5(8) . . . . ? C27 C28 C29 C30 -1.4(15) . . . . ? C28 C29 C30 F30 -179.9(8) . . . . ? F29 C29 C30 F30 -0.7(13) . . . . ? C28 C29 C30 C25 0.3(14) . . . . ? F29 C29 C30 C25 179.4(8) . . . . ? C26 C25 C30 F30 -178.2(7) . . . . ? S2 C25 C30 F30 -5.5(11) . . . . ? C26 C25 C30 C29 1.6(12) . . . . ? S2 C25 C30 C29 174.3(7) . . . . ? Pt1 S3 C31 C36 -135.4(7) . . . . ? Pt1 S3 C31 C32 45.9(9) . . . . ? C36 C31 C32 F32 -175.6(9) . . . . ? S3 C31 C32 F32 3.2(13) . . . . ? C36 C31 C32 C33 0.9(15) . . . . ? S3 C31 C32 C33 179.7(8) . . . . ? F32 C32 C33 C34 176.2(12) . . . . ? C31 C32 C33 C34 -0.3(19) . . . . ? F32 C32 C33 F33 -1.5(16) . . . . ? C31 C32 C33 F33 -178.0(10) . . . . ? F33 C33 C34 C35 177.5(13) . . . . ? C32 C33 C34 C35 0(2) . . . . ? C33 C34 C35 F35 -179.2(12) . . . . ? C33 C34 C35 C36 0(2) . . . . ? F35 C35 C36 F36 1.2(17) . . . . ? C34 C35 C36 F36 -178.1(12) . . . . ? F35 C35 C36 C31 179.9(10) . . . . ? C34 C35 C36 C31 1(2) . . . . ? C32 C31 C36 F36 177.7(9) . . . . ? S3 C31 C36 F36 -1.2(13) . . . . ? C32 C31 C36 C35 -1.0(15) . . . . ? S3 C31 C36 C35 -179.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.266 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.137 ######################################################## # End of Crystallographic Information File (CIF) # ######################################################## data_lv104-3 _database_code_depnum_ccdc_archive 'CCDC 239573' _audit_creation_method SHELXL-97 _audit_creation_date 2003-06-02 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H8 F21 P Pt S3' _chemical_formula_sum 'C36 H8 F21 P Pt S3' _chemical_formula_weight 1161.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8338(10) _cell_length_b 12.4575(14) _cell_length_c 14.5848(13) _cell_angle_alpha 96.898(8) _cell_angle_beta 107.898(7) _cell_angle_gamma 105.595(7) _cell_volume 1921.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(1) _cell_measurement_reflns_used 88 _cell_measurement_theta_min 4.70 _cell_measurement_theta_max 13.01 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 3.986 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.480 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details '50 psi scans with XSCAnS 2.21 (Fait, 1996)' _exptl_special_details ? _diffrn_ambient_temperature 296(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_source_power 1.5 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_detector 'Scintillation counter' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 0 0 2 -1 3 -2 -2 1 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 13307 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6727 _reflns_number_gt 5688 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'XSCAnS 2.21 (Fait, 1996)' _computing_cell_refinement 'XSCAnS 2.21 (Fait, 1996)' _computing_data_reduction 'XSCAnS 2.21 (Fait, 1996)' _computing_structure_solution 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.10 (Sheldrick, 1998)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+1.0207P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6727 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.152004(16) 0.184248(15) 0.195152(16) 0.04798(9) Uani 1 1 d . . . P1 P 1.29295(12) 0.12814(11) 0.30165(11) 0.0548(3) Uani 1 1 d . . . S1 S 1.17821(12) 0.08099(11) 0.06765(11) 0.0559(3) Uani 1 1 d . . . S2 S 1.13357(13) 0.29202(13) 0.32656(12) 0.0667(4) Uani 1 1 d . . . S3 S 1.00155(13) 0.22678(12) 0.06961(11) 0.0605(4) Uani 1 1 d . . . C1 C 1.2982(4) 0.0236(4) 0.1247(5) 0.0548(14) Uani 1 1 d . . . C2 C 1.3416(5) 0.0335(4) 0.2266(5) 0.0574(14) Uani 1 1 d . . . C3 C 1.4220(5) -0.0266(5) 0.2637(5) 0.0700(17) Uani 1 1 d . . . C4 C 1.4583(6) -0.0925(5) 0.2030(7) 0.079(2) Uani 1 1 d . . . C5 C 1.4189(6) -0.0977(5) 0.1044(7) 0.0774(19) Uani 1 1 d . . . C6 C 1.3367(5) -0.0421(5) 0.0637(5) 0.0661(16) Uani 1 1 d . . . C7 C 1.2537(5) 0.1758(5) 0.0070(5) 0.0634(15) Uani 1 1 d . . . C8 C 1.3706(6) 0.2574(5) 0.0522(5) 0.0672(16) Uani 1 1 d . . . C9 C 1.4227(7) 0.3256(6) 0.0005(8) 0.088(2) Uani 1 1 d . . . C10 C 1.3591(11) 0.3184(8) -0.0968(8) 0.103(3) Uani 1 1 d . . . H10A H 1.3946 0.3667 -0.1316 0.123 Uiso 1 1 calc R . . C11 C 1.2429(11) 0.2393(8) -0.1420(6) 0.103(3) Uani 1 1 d . . . C12 C 1.1891(7) 0.1679(6) -0.0927(5) 0.0785(19) Uani 1 1 d . . . C13 C 1.4361(5) 0.2389(5) 0.3831(5) 0.0716(17) Uani 1 1 d . . . C14 C 1.5217(8) 0.2190(8) 0.4621(7) 0.123(3) Uani 1 1 d . . . H14A H 1.5083 0.1465 0.4755 0.147 Uiso 1 1 calc R . . C15 C 1.6285(9) 0.3091(10) 0.5214(9) 0.157(5) Uani 1 1 d . . . H15A H 1.6859 0.2975 0.5761 0.189 Uiso 1 1 calc R . . C16 C 1.6496(8) 0.4167(10) 0.4989(9) 0.147(5) Uani 1 1 d . . . H16A H 1.7232 0.4760 0.5359 0.176 Uiso 1 1 calc R . . C17 C 1.5627(7) 0.4337(7) 0.4236(7) 0.104(3) Uani 1 1 d . . . H17A H 1.5745 0.5069 0.4117 0.124 Uiso 1 1 calc R . . C18 C 1.4569(5) 0.3468(5) 0.3635(5) 0.0765(18) Uani 1 1 d . . . H18A H 1.3997 0.3603 0.3100 0.092 Uiso 1 1 calc R . . C19 C 1.2305(6) 0.0406(5) 0.3785(5) 0.0670(15) Uani 1 1 d . . . C20 C 1.1660(6) -0.0742(6) 0.3436(5) 0.0724(16) Uani 1 1 d . . . C21 C 1.1105(8) -0.1434(7) 0.3951(7) 0.095(2) Uani 1 1 d . . . C22 C 1.1137(10) -0.0956(10) 0.4836(8) 0.114(3) Uani 1 1 d . . . C23 C 1.1747(10) 0.0196(10) 0.5230(6) 0.111(3) Uani 1 1 d . . . C24 C 1.2317(8) 0.0866(7) 0.4702(5) 0.088(2) Uani 1 1 d . . . C25 C 0.9789(5) 0.2955(4) 0.2978(4) 0.0540(13) Uani 1 1 d . . . C26 C 0.9606(5) 0.3999(5) 0.3184(5) 0.0663(16) Uani 1 1 d . . . C27 C 0.8429(7) 0.4088(7) 0.3059(6) 0.091(2) Uani 1 1 d . . . C28 C 0.7419(7) 0.3147(8) 0.2730(6) 0.103(3) Uani 1 1 d . . . H28A H 0.6631 0.3197 0.2672 0.124 Uiso 1 1 calc R . . C29 C 0.7558(6) 0.2120(7) 0.2483(6) 0.089(2) Uani 1 1 d . . . C30 C 0.8737(6) 0.2017(5) 0.2620(5) 0.0673(16) Uani 1 1 d . . . C31 C 1.0281(6) 0.3737(5) 0.1010(4) 0.0611(14) Uani 1 1 d . . . C32 C 1.1434(7) 0.4564(5) 0.1365(5) 0.0746(17) Uani 1 1 d . . . C33 C 1.1576(10) 0.5708(6) 0.1580(6) 0.106(3) Uani 1 1 d . . . C34 C 1.0518(13) 0.6063(7) 0.1423(7) 0.118(4) Uani 1 1 d . . . H34A H 1.0597 0.6834 0.1566 0.141 Uiso 1 1 calc R . . C35 C 0.9409(11) 0.5270(8) 0.1067(6) 0.105(3) Uani 1 1 d . . . C36 C 0.9252(7) 0.4115(6) 0.0873(5) 0.0747(18) Uani 1 1 d . . . F3 F 1.4621(4) -0.0257(4) 0.3612(3) 0.0972(13) Uani 1 1 d . . . F4 F 1.5361(4) -0.1491(4) 0.2435(4) 0.1137(16) Uani 1 1 d . . . F5 F 1.4580(4) -0.1583(4) 0.0464(4) 0.1078(15) Uani 1 1 d . . . F6 F 1.2986(3) -0.0475(3) -0.0327(3) 0.0853(11) Uani 1 1 d . . . F8 F 1.4340(3) 0.2664(3) 0.1482(3) 0.0851(11) Uani 1 1 d . . . F9 F 1.5375(5) 0.4019(4) 0.0471(5) 0.1265(19) Uani 1 1 d . . . F11 F 1.1785(7) 0.2306(5) -0.2372(4) 0.155(2) Uani 1 1 d . . . F12 F 1.0739(5) 0.0922(4) -0.1383(3) 0.1085(15) Uani 1 1 d . . . F20 F 1.1555(4) -0.1262(3) 0.2532(3) 0.0933(12) Uani 1 1 d . . . F21 F 1.0530(6) -0.2549(4) 0.3582(5) 0.1350(19) Uani 1 1 d . . . F22 F 1.0551(7) -0.1580(6) 0.5340(5) 0.174(3) Uani 1 1 d . . . F23 F 1.1757(7) 0.0704(7) 0.6102(4) 0.172(3) Uani 1 1 d . . . F24 F 1.2899(5) 0.1984(4) 0.5110(3) 0.1166(15) Uani 1 1 d . . . F26 F 1.0595(3) 0.4970(3) 0.3542(4) 0.0928(12) Uani 1 1 d . . . F27 F 0.8339(5) 0.5135(5) 0.3288(5) 0.146(2) Uani 1 1 d . . . F29 F 0.6555(4) 0.1161(5) 0.2147(5) 0.150(2) Uani 1 1 d . . . F30 F 0.8835(4) 0.0972(3) 0.2422(3) 0.0968(13) Uani 1 1 d . . . F32 F 1.2491(4) 0.4268(4) 0.1506(4) 0.1049(14) Uani 1 1 d . . . F33 F 1.2737(6) 0.6470(4) 0.1910(5) 0.167(3) Uani 1 1 d . . . F35 F 0.8347(7) 0.5564(5) 0.0883(5) 0.158(3) Uani 1 1 d . . . F36 F 0.8082(4) 0.3354(4) 0.0501(4) 0.1020(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03889(11) 0.04053(12) 0.05807(14) -0.00135(8) 0.00940(8) 0.01707(8) P1 0.0465(7) 0.0490(7) 0.0594(9) -0.0005(6) 0.0066(6) 0.0201(6) S1 0.0450(7) 0.0526(7) 0.0605(8) -0.0050(6) 0.0086(6) 0.0197(6) S2 0.0531(8) 0.0741(9) 0.0625(9) -0.0117(7) 0.0060(7) 0.0324(7) S3 0.0512(7) 0.0562(8) 0.0642(9) -0.0002(7) 0.0050(6) 0.0260(6) C1 0.040(3) 0.041(3) 0.078(4) 0.000(3) 0.016(3) 0.017(2) C2 0.042(3) 0.045(3) 0.079(4) 0.006(3) 0.013(3) 0.018(2) C3 0.056(3) 0.065(4) 0.088(5) 0.019(3) 0.017(3) 0.028(3) C4 0.055(3) 0.056(3) 0.130(7) 0.011(4) 0.027(4) 0.035(3) C5 0.061(4) 0.056(3) 0.117(6) 0.000(4) 0.035(4) 0.026(3) C6 0.059(3) 0.052(3) 0.081(5) -0.005(3) 0.021(3) 0.021(3) C7 0.067(4) 0.060(3) 0.071(4) 0.007(3) 0.025(3) 0.037(3) C8 0.066(4) 0.069(4) 0.082(5) 0.020(3) 0.031(4) 0.038(3) C9 0.085(5) 0.072(4) 0.139(8) 0.038(5) 0.060(5) 0.043(4) C10 0.156(9) 0.101(6) 0.121(8) 0.057(6) 0.088(7) 0.091(7) C11 0.164(9) 0.096(6) 0.081(6) 0.025(5) 0.048(6) 0.088(6) C12 0.103(5) 0.077(4) 0.068(4) 0.011(4) 0.025(4) 0.058(4) C13 0.053(3) 0.064(4) 0.081(4) -0.008(3) 0.006(3) 0.022(3) C14 0.088(5) 0.104(6) 0.120(7) -0.019(5) -0.033(5) 0.043(5) C15 0.095(7) 0.128(8) 0.163(10) -0.046(8) -0.053(6) 0.049(6) C16 0.057(5) 0.133(9) 0.171(10) -0.072(8) -0.016(6) 0.016(5) C17 0.065(5) 0.078(5) 0.132(7) -0.025(5) 0.028(5) -0.003(4) C18 0.052(3) 0.063(4) 0.097(5) -0.014(3) 0.020(3) 0.011(3) C19 0.064(3) 0.069(4) 0.064(4) 0.010(3) 0.012(3) 0.030(3) C20 0.071(4) 0.072(4) 0.072(4) 0.018(4) 0.023(3) 0.023(3) C21 0.105(6) 0.086(5) 0.094(6) 0.032(5) 0.036(5) 0.027(5) C22 0.127(7) 0.131(8) 0.097(7) 0.056(7) 0.049(6) 0.038(6) C23 0.131(7) 0.152(9) 0.064(5) 0.031(6) 0.043(5) 0.057(7) C24 0.107(6) 0.089(5) 0.067(5) 0.006(4) 0.023(4) 0.045(4) C25 0.050(3) 0.056(3) 0.054(3) 0.005(3) 0.017(2) 0.020(2) C26 0.052(3) 0.062(3) 0.086(4) 0.003(3) 0.028(3) 0.021(3) C27 0.068(4) 0.093(5) 0.116(6) 0.000(4) 0.035(4) 0.041(4) C28 0.060(4) 0.143(8) 0.105(6) -0.006(5) 0.035(4) 0.037(5) C29 0.049(3) 0.099(5) 0.092(5) -0.010(4) 0.032(4) -0.013(4) C30 0.075(4) 0.056(3) 0.067(4) 0.002(3) 0.033(3) 0.009(3) C31 0.075(4) 0.059(3) 0.058(3) 0.017(3) 0.023(3) 0.034(3) C32 0.086(5) 0.063(4) 0.067(4) 0.014(3) 0.013(3) 0.029(3) C33 0.150(8) 0.053(4) 0.079(5) 0.012(4) 0.011(5) 0.014(5) C34 0.210(12) 0.059(5) 0.086(6) 0.017(4) 0.040(7) 0.062(6) C35 0.180(9) 0.094(6) 0.087(6) 0.033(5) 0.057(6) 0.098(7) C36 0.096(5) 0.075(4) 0.067(4) 0.020(3) 0.027(4) 0.050(4) F3 0.096(3) 0.105(3) 0.103(3) 0.035(3) 0.020(2) 0.065(3) F4 0.097(3) 0.105(3) 0.166(5) 0.037(3) 0.041(3) 0.079(3) F5 0.096(3) 0.091(3) 0.151(4) -0.007(3) 0.053(3) 0.056(2) F6 0.081(2) 0.080(2) 0.090(3) -0.016(2) 0.032(2) 0.0305(19) F8 0.0545(19) 0.085(2) 0.096(3) 0.015(2) 0.0122(19) 0.0109(18) F9 0.101(3) 0.101(3) 0.206(6) 0.062(4) 0.078(4) 0.037(3) F11 0.260(7) 0.155(5) 0.077(4) 0.040(3) 0.047(4) 0.117(5) F12 0.117(3) 0.102(3) 0.070(3) -0.013(2) -0.010(2) 0.043(3) F20 0.112(3) 0.061(2) 0.095(3) 0.001(2) 0.048(2) 0.003(2) F21 0.161(5) 0.086(3) 0.165(5) 0.052(3) 0.076(4) 0.021(3) F22 0.210(7) 0.200(6) 0.135(5) 0.094(5) 0.093(5) 0.044(5) F23 0.230(7) 0.226(7) 0.089(4) 0.027(4) 0.085(5) 0.089(6) F24 0.153(4) 0.106(3) 0.079(3) -0.010(2) 0.030(3) 0.049(3) F26 0.069(2) 0.056(2) 0.141(4) -0.007(2) 0.032(2) 0.0189(18) F27 0.112(4) 0.118(4) 0.226(7) 0.003(4) 0.063(4) 0.077(3) F29 0.084(3) 0.149(5) 0.165(5) -0.028(4) 0.064(3) -0.039(3) F30 0.119(3) 0.056(2) 0.107(3) 0.001(2) 0.053(3) 0.006(2) F32 0.069(2) 0.091(3) 0.130(4) 0.032(3) 0.013(2) 0.008(2) F33 0.186(6) 0.068(3) 0.158(5) 0.022(3) -0.006(4) -0.020(3) F35 0.230(7) 0.156(5) 0.182(6) 0.065(4) 0.104(5) 0.161(5) F36 0.083(3) 0.118(3) 0.131(4) 0.041(3) 0.039(3) 0.066(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2313(14) . ? Pt1 S1 2.2812(14) . ? Pt1 S2 2.3064(15) . ? Pt1 S3 2.3537(14) . ? P1 C13 1.815(6) . ? P1 C2 1.833(6) . ? P1 C19 1.833(7) . ? S1 C7 1.773(6) . ? S1 C1 1.784(5) . ? S2 C25 1.761(5) . ? S3 C31 1.750(6) . ? C1 C2 1.392(8) . ? C1 C6 1.394(8) . ? C2 C3 1.388(8) . ? C3 F3 1.352(8) . ? C3 C4 1.374(9) . ? C4 F4 1.345(7) . ? C4 C5 1.356(10) . ? C5 F5 1.333(8) . ? C5 C6 1.372(9) . ? C6 F6 1.325(8) . ? C7 C8 1.380(8) . ? C7 C12 1.397(9) . ? C8 F8 1.344(7) . ? C8 C9 1.353(10) . ? C9 F9 1.339(9) . ? C9 C10 1.366(12) . ? C10 C11 1.361(12) . ? C10 H10A 0.9300 . ? C11 F11 1.338(10) . ? C11 C12 1.357(12) . ? C12 F12 1.338(8) . ? C13 C14 1.379(10) . ? C13 C18 1.381(9) . ? C14 C15 1.392(12) . ? C14 H14A 0.9300 . ? C15 C16 1.393(16) . ? C15 H15A 0.9300 . ? C16 C17 1.337(14) . ? C16 H16A 0.9300 . ? C17 C18 1.370(9) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.373(9) . ? C19 C24 1.385(9) . ? C20 F20 1.351(8) . ? C20 C21 1.376(10) . ? C21 F21 1.329(9) . ? C21 C22 1.340(13) . ? C22 F22 1.336(10) . ? C22 C23 1.379(13) . ? C23 F23 1.345(10) . ? C23 C24 1.384(12) . ? C24 F24 1.342(8) . ? C25 C30 1.364(8) . ? C25 C26 1.389(8) . ? C26 F26 1.347(7) . ? C26 C27 1.384(8) . ? C27 C28 1.339(11) . ? C27 F27 1.347(8) . ? C28 C29 1.353(11) . ? C28 H28A 0.9300 . ? C29 F29 1.348(7) . ? C29 C30 1.391(10) . ? C30 F30 1.343(7) . ? C31 C32 1.368(9) . ? C31 C36 1.387(8) . ? C32 F32 1.361(8) . ? C32 C33 1.374(10) . ? C33 F33 1.343(10) . ? C33 C34 1.400(14) . ? C34 C35 1.315(13) . ? C34 H34A 0.9300 . ? C35 F35 1.360(10) . ? C35 C36 1.383(10) . ? C36 F36 1.348(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 S1 89.41(5) . . ? P1 Pt1 S2 89.29(5) . . ? S1 Pt1 S2 177.84(5) . . ? P1 Pt1 S3 173.74(5) . . ? S1 Pt1 S3 84.62(5) . . ? S2 Pt1 S3 96.74(5) . . ? C13 P1 C2 106.0(3) . . ? C13 P1 C19 107.5(3) . . ? C2 P1 C19 104.9(3) . . ? C13 P1 Pt1 116.9(2) . . ? C2 P1 Pt1 106.10(19) . . ? C19 P1 Pt1 114.49(19) . . ? C7 S1 C1 101.4(3) . . ? C7 S1 Pt1 109.28(19) . . ? C1 S1 Pt1 105.2(2) . . ? C25 S2 Pt1 110.52(19) . . ? C31 S3 Pt1 107.0(2) . . ? C2 C1 C6 121.0(5) . . ? C2 C1 S1 120.6(4) . . ? C6 C1 S1 118.0(5) . . ? C3 C2 C1 117.0(5) . . ? C3 C2 P1 125.0(5) . . ? C1 C2 P1 118.0(4) . . ? F3 C3 C4 118.3(6) . . ? F3 C3 C2 119.9(6) . . ? C4 C3 C2 121.7(7) . . ? F4 C4 C5 120.7(6) . . ? F4 C4 C3 118.8(8) . . ? C5 C4 C3 120.4(6) . . ? F5 C5 C4 120.3(6) . . ? F5 C5 C6 119.6(8) . . ? C4 C5 C6 120.1(6) . . ? F6 C6 C5 119.8(6) . . ? F6 C6 C1 120.5(5) . . ? C5 C6 C1 119.7(7) . . ? C8 C7 C12 118.3(6) . . ? C8 C7 S1 124.3(5) . . ? C12 C7 S1 117.4(5) . . ? F8 C8 C9 120.1(7) . . ? F8 C8 C7 119.1(6) . . ? C9 C8 C7 120.8(7) . . ? F9 C9 C8 118.6(8) . . ? F9 C9 C10 120.5(8) . . ? C8 C9 C10 120.9(8) . . ? C11 C10 C9 118.9(8) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? F11 C11 C10 120.1(10) . . ? F11 C11 C12 118.2(10) . . ? C10 C11 C12 121.7(8) . . ? F12 C12 C11 120.6(8) . . ? F12 C12 C7 119.9(7) . . ? C11 C12 C7 119.5(8) . . ? C14 C13 C18 120.1(6) . . ? C14 C13 P1 122.8(6) . . ? C18 C13 P1 117.2(5) . . ? C13 C14 C15 119.1(9) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C14 C15 C16 120.0(9) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 119.3(8) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C16 C17 C18 122.0(9) . . ? C16 C17 H17A 119.0 . . ? C18 C17 H17A 119.0 . . ? C17 C18 C13 119.4(7) . . ? C17 C18 H18A 120.3 . . ? C13 C18 H18A 120.3 . . ? C20 C19 C24 115.1(6) . . ? C20 C19 P1 121.6(5) . . ? C24 C19 P1 122.9(5) . . ? F20 C20 C19 119.6(6) . . ? F20 C20 C21 115.8(6) . . ? C19 C20 C21 124.6(7) . . ? F21 C21 C22 120.1(8) . . ? F21 C21 C20 121.5(8) . . ? C22 C21 C20 118.4(8) . . ? F22 C22 C21 120.6(10) . . ? F22 C22 C23 118.9(10) . . ? C21 C22 C23 120.5(8) . . ? F23 C23 C22 121.6(9) . . ? F23 C23 C24 118.6(10) . . ? C22 C23 C24 119.7(8) . . ? F24 C24 C19 120.5(7) . . ? F24 C24 C23 117.9(7) . . ? C19 C24 C23 121.6(8) . . ? C30 C25 C26 116.2(5) . . ? C30 C25 S2 125.0(4) . . ? C26 C25 S2 118.7(4) . . ? F26 C26 C27 117.7(6) . . ? F26 C26 C25 120.1(5) . . ? C27 C26 C25 122.2(6) . . ? C28 C27 F27 121.7(6) . . ? C28 C27 C26 120.0(7) . . ? F27 C27 C26 118.3(7) . . ? C27 C28 C29 119.2(6) . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? F29 C29 C28 120.3(7) . . ? F29 C29 C30 118.3(7) . . ? C28 C29 C30 121.3(6) . . ? F30 C30 C25 119.9(6) . . ? F30 C30 C29 119.1(6) . . ? C25 C30 C29 121.0(6) . . ? C32 C31 C36 116.4(6) . . ? C32 C31 S3 125.2(5) . . ? C36 C31 S3 118.4(5) . . ? F32 C32 C31 120.2(5) . . ? F32 C32 C33 117.6(7) . . ? C31 C32 C33 122.3(7) . . ? F33 C33 C32 118.8(9) . . ? F33 C33 C34 121.1(8) . . ? C32 C33 C34 120.0(8) . . ? C35 C34 C33 117.7(7) . . ? C35 C34 H34A 121.1 . . ? C33 C34 H34A 121.1 . . ? C34 C35 F35 120.4(8) . . ? C34 C35 C36 122.9(8) . . ? F35 C35 C36 116.7(10) . . ? F36 C36 C35 119.4(7) . . ? F36 C36 C31 119.9(6) . . ? C35 C36 C31 120.6(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Pt1 P1 C13 116.7(3) . . . . ? S2 Pt1 P1 C13 -61.6(3) . . . . ? S3 Pt1 P1 C13 134.3(5) . . . . ? S1 Pt1 P1 C2 -1.22(18) . . . . ? S2 Pt1 P1 C2 -179.50(18) . . . . ? S3 Pt1 P1 C2 16.4(6) . . . . ? S1 Pt1 P1 C19 -116.4(2) . . . . ? S2 Pt1 P1 C19 65.3(2) . . . . ? S3 Pt1 P1 C19 -98.8(5) . . . . ? P1 Pt1 S1 C7 -111.2(2) . . . . ? S2 Pt1 S1 C7 -58.2(15) . . . . ? S3 Pt1 S1 C7 70.7(2) . . . . ? P1 Pt1 S1 C1 -3.01(18) . . . . ? S2 Pt1 S1 C1 50.0(15) . . . . ? S3 Pt1 S1 C1 178.89(18) . . . . ? P1 Pt1 S2 C25 -146.5(2) . . . . ? S1 Pt1 S2 C25 160.5(14) . . . . ? S3 Pt1 S2 C25 31.8(2) . . . . ? P1 Pt1 S3 C31 -151.8(5) . . . . ? S1 Pt1 S3 C31 -134.1(2) . . . . ? S2 Pt1 S3 C31 44.2(2) . . . . ? C7 S1 C1 C2 122.5(5) . . . . ? Pt1 S1 C1 C2 8.6(5) . . . . ? C7 S1 C1 C6 -64.6(5) . . . . ? Pt1 S1 C1 C6 -178.4(4) . . . . ? C6 C1 C2 C3 -1.4(8) . . . . ? S1 C1 C2 C3 171.3(4) . . . . ? C6 C1 C2 P1 176.6(4) . . . . ? S1 C1 C2 P1 -10.7(6) . . . . ? C13 P1 C2 C3 59.9(6) . . . . ? C19 P1 C2 C3 -53.7(5) . . . . ? Pt1 P1 C2 C3 -175.2(4) . . . . ? C13 P1 C2 C1 -118.0(5) . . . . ? C19 P1 C2 C1 128.5(4) . . . . ? Pt1 P1 C2 C1 6.9(4) . . . . ? C1 C2 C3 F3 -176.4(5) . . . . ? P1 C2 C3 F3 5.8(8) . . . . ? C1 C2 C3 C4 0.5(9) . . . . ? P1 C2 C3 C4 -177.3(5) . . . . ? F3 C3 C4 F4 -2.8(9) . . . . ? C2 C3 C4 F4 -179.7(6) . . . . ? F3 C3 C4 C5 178.9(6) . . . . ? C2 C3 C4 C5 2.0(10) . . . . ? F4 C4 C5 F5 -0.7(10) . . . . ? C3 C4 C5 F5 177.6(6) . . . . ? F4 C4 C5 C6 178.1(6) . . . . ? C3 C4 C5 C6 -3.6(10) . . . . ? F5 C5 C6 F6 -1.1(9) . . . . ? C4 C5 C6 F6 180.0(6) . . . . ? F5 C5 C6 C1 -178.4(5) . . . . ? C4 C5 C6 C1 2.7(9) . . . . ? C2 C1 C6 F6 -177.4(5) . . . . ? S1 C1 C6 F6 9.6(7) . . . . ? C2 C1 C6 C5 -0.2(9) . . . . ? S1 C1 C6 C5 -173.1(5) . . . . ? C1 S1 C7 C8 -51.1(5) . . . . ? Pt1 S1 C7 C8 59.6(5) . . . . ? C1 S1 C7 C12 130.0(4) . . . . ? Pt1 S1 C7 C12 -119.3(4) . . . . ? C12 C7 C8 F8 179.8(5) . . . . ? S1 C7 C8 F8 0.9(7) . . . . ? C12 C7 C8 C9 -2.0(8) . . . . ? S1 C7 C8 C9 179.1(5) . . . . ? F8 C8 C9 F9 -0.4(9) . . . . ? C7 C8 C9 F9 -178.6(5) . . . . ? F8 C8 C9 C10 -179.4(6) . . . . ? C7 C8 C9 C10 2.5(10) . . . . ? F9 C9 C10 C11 179.6(6) . . . . ? C8 C9 C10 C11 -1.5(11) . . . . ? C9 C10 C11 F11 179.9(6) . . . . ? C9 C10 C11 C12 0.0(11) . . . . ? F11 C11 C12 F12 -1.0(10) . . . . ? C10 C11 C12 F12 178.9(6) . . . . ? F11 C11 C12 C7 -179.4(6) . . . . ? C10 C11 C12 C7 0.4(10) . . . . ? C8 C7 C12 F12 -177.9(5) . . . . ? S1 C7 C12 F12 1.1(7) . . . . ? C8 C7 C12 C11 0.5(9) . . . . ? S1 C7 C12 C11 179.6(5) . . . . ? C2 P1 C13 C14 -72.4(7) . . . . ? C19 P1 C13 C14 39.4(8) . . . . ? Pt1 P1 C13 C14 169.7(6) . . . . ? C2 P1 C13 C18 108.0(5) . . . . ? C19 P1 C13 C18 -140.2(5) . . . . ? Pt1 P1 C13 C18 -9.9(6) . . . . ? C18 C13 C14 C15 0.2(14) . . . . ? P1 C13 C14 C15 -179.4(8) . . . . ? C13 C14 C15 C16 -1.9(18) . . . . ? C14 C15 C16 C17 3.9(19) . . . . ? C15 C16 C17 C18 -4.3(16) . . . . ? C16 C17 C18 C13 2.6(12) . . . . ? C14 C13 C18 C17 -0.5(11) . . . . ? P1 C13 C18 C17 179.1(5) . . . . ? C13 P1 C19 C20 -147.7(5) . . . . ? C2 P1 C19 C20 -35.1(6) . . . . ? Pt1 P1 C19 C20 80.8(5) . . . . ? C13 P1 C19 C24 40.0(6) . . . . ? C2 P1 C19 C24 152.5(6) . . . . ? Pt1 P1 C19 C24 -91.6(6) . . . . ? C24 C19 C20 F20 177.6(6) . . . . ? P1 C19 C20 F20 4.7(9) . . . . ? C24 C19 C20 C21 -3.2(10) . . . . ? P1 C19 C20 C21 -176.1(6) . . . . ? F20 C20 C21 F21 1.5(11) . . . . ? C19 C20 C21 F21 -177.7(7) . . . . ? F20 C20 C21 C22 -177.4(8) . . . . ? C19 C20 C21 C22 3.4(12) . . . . ? F21 C21 C22 F22 -2.7(15) . . . . ? C20 C21 C22 F22 176.2(8) . . . . ? F21 C21 C22 C23 179.1(9) . . . . ? C20 C21 C22 C23 -2.0(15) . . . . ? F22 C22 C23 F23 -0.4(15) . . . . ? C21 C22 C23 F23 177.8(9) . . . . ? F22 C22 C23 C24 -177.5(8) . . . . ? C21 C22 C23 C24 0.7(16) . . . . ? C20 C19 C24 F24 -178.8(6) . . . . ? P1 C19 C24 F24 -6.0(10) . . . . ? C20 C19 C24 C23 1.8(11) . . . . ? P1 C19 C24 C23 174.6(6) . . . . ? F23 C23 C24 F24 2.7(13) . . . . ? C22 C23 C24 F24 179.9(8) . . . . ? F23 C23 C24 C19 -177.8(7) . . . . ? C22 C23 C24 C19 -0.6(14) . . . . ? Pt1 S2 C25 C30 51.7(6) . . . . ? Pt1 S2 C25 C26 -132.8(5) . . . . ? C30 C25 C26 F26 179.9(6) . . . . ? S2 C25 C26 F26 4.0(8) . . . . ? C30 C25 C26 C27 1.5(10) . . . . ? S2 C25 C26 C27 -174.4(6) . . . . ? F26 C26 C27 C28 -178.3(7) . . . . ? C25 C26 C27 C28 0.2(13) . . . . ? F26 C26 C27 F27 0.8(12) . . . . ? C25 C26 C27 F27 179.3(7) . . . . ? F27 C27 C28 C29 178.1(8) . . . . ? C26 C27 C28 C29 -2.8(14) . . . . ? C27 C28 C29 F29 -179.7(8) . . . . ? C27 C28 C29 C30 3.9(13) . . . . ? C26 C25 C30 F30 -178.6(6) . . . . ? S2 C25 C30 F30 -3.0(9) . . . . ? C26 C25 C30 C29 -0.5(9) . . . . ? S2 C25 C30 C29 175.2(5) . . . . ? F29 C29 C30 F30 -0.5(10) . . . . ? C28 C29 C30 F30 175.9(7) . . . . ? F29 C29 C30 C25 -178.7(6) . . . . ? C28 C29 C30 C25 -2.2(12) . . . . ? Pt1 S3 C31 C32 43.3(6) . . . . ? Pt1 S3 C31 C36 -138.2(5) . . . . ? C36 C31 C32 F32 -179.0(6) . . . . ? S3 C31 C32 F32 -0.5(9) . . . . ? C36 C31 C32 C33 0.2(10) . . . . ? S3 C31 C32 C33 178.7(6) . . . . ? F32 C32 C33 F33 0.4(11) . . . . ? C31 C32 C33 F33 -178.8(7) . . . . ? F32 C32 C33 C34 178.3(7) . . . . ? C31 C32 C33 C34 -0.9(12) . . . . ? F33 C33 C34 C35 177.7(8) . . . . ? C32 C33 C34 C35 -0.2(13) . . . . ? C33 C34 C35 F35 -178.9(8) . . . . ? C33 C34 C35 C36 2.1(14) . . . . ? C34 C35 C36 F36 -179.6(8) . . . . ? F35 C35 C36 F36 1.3(11) . . . . ? C34 C35 C36 C31 -2.9(12) . . . . ? F35 C35 C36 C31 178.0(7) . . . . ? C32 C31 C36 F36 178.3(6) . . . . ? S3 C31 C36 F36 -0.4(9) . . . . ? C32 C31 C36 C35 1.6(10) . . . . ? S3 C31 C36 C35 -177.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.595 _refine_diff_density_min -1.253 _refine_diff_density_rms 0.088 ######################################################## # End of Crystallographic Information File (CIF) # ########################################################